Methanol → 3-Methoxy-2-methylpyridine

HRID 128612Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 128612
[CH3:1][O-].[Na+].CO.[OH:6][C:7]1[C:8]([CH3:13])=[N:9][CH:10]=[CH:11][CH:12]=1>CN(C=O)C>[CH3:1][O:6][C:7]1[C:8]([CH3:13])=[N:9][CH:10]=[CH:11][CH:12]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 707192-Methylpyridin-3-olHCID 10942334Sodium Methoxide

Produkt 1

HCID 30152703-Methoxy-2-methylpyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of sodium methoxide (prepared from sodium metal) (10.2 g) and methanol (175 ml), 3-hydroxy-2-methylpyridine (43.0 g) phenyltrimethylammonium chloride (81.9 g) and DMF (400 ml) was boiled under reflux with stirring for 5 hours under nitrogen. The mixture was filtered and distilled. The fraction boiling at 167°-195° C. was collected and purified by flash chromatography on silica using dichloromethane and then IMS as the mobile phase to give 3-methoxy-2-methylpyridine which was used without further purification.

Aufarbeitung

  1. temperatureunder reflux
  2. filtrationThe mixture was filtered
  3. distillationdistilled
  4. customThe fraction boiling at 167°-195° C. was collected
  5. custompurified by flash chromatography on silica

Quellen und Nachweise

ORD-Eintrag
ord-9e78cd18ee884424b76f8b82d9556edd
Quelldatensatz
uspto-grants-1995_11
Patentnummer
US05464781

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